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The activation of iron oxide Fischer-Tropsch Synthesis(FTS)catalysts was investigated during pretreat-ment:reduction in hydrogen followed by carburization in either CO or syngas mixture,or simultaneously reduction and carburization in syngas.A combination of different complementary in situ techniques was used to gain insight into the behavior of Fe-based FTS catalysts during activation.In situ XRD was used to identify the crystalline structures present during both reduction in hydrogen and carburization.An increase in reduction rate was established when increasing the temperature.A complete reduction was demonstrated in the ETEM and a grain size dependency was proven,i.e.bigger grains need higher tem-perature in order to reduce.XPS and XAS both indicate the formation of a small amount of carbonaceous species at the surface of the bulk metallic iron during carburization.